CN110055523A - Water base silver protecting agent and preparation method thereof - Google Patents
Water base silver protecting agent and preparation method thereof Download PDFInfo
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- CN110055523A CN110055523A CN201910326145.3A CN201910326145A CN110055523A CN 110055523 A CN110055523 A CN 110055523A CN 201910326145 A CN201910326145 A CN 201910326145A CN 110055523 A CN110055523 A CN 110055523A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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Abstract
The present invention provides a kind of water base silver protecting agents and preparation method thereof.A kind of water base silver protecting agent, every liter of water base silver protecting agent include: Stearyl mercaptan 40-60g, trimethyl sulfydryl phosphate 4-10g, emulsifier 20-60g, coupling agent 2-5g, silica 5-10g, stabilizer 10-15g, and surplus is water.A kind of protectant preparation method of water based silver, comprising the following steps: Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water and are mixed to get component A；Coupling agent and silica are added to the water and are mixed to get B component；Emulsifier and stabilizer are added to the water and are mixed to get component C；A, B, component C are mixed to obtain water base silver protecting agent.Water base silver protecting agent provided by the present application, improves adhesive force and wearability, to improve the corrosion resistance and discoloration-resisting of electronic connector, so that the resistance to 5% potassium sulfide test period of electronic connector extends, guard time is greatly improved.
Description
Technical field
The present invention relates to field of surface treatment, in particular to a kind of water base silver protecting agent and preparation method thereof.
Background technique
Metallic silver with its excellent performance and relatively low price become the noble metal that is most widely used at present it
One, silver has good electric conductivity, thermal conductance, soldering property, corrosion resistance and stability in each metal, therefore metallic silver is logical
News, electronics, the application in electric product are especially extensive.But silver belongs to noble metal after all, so silver is improved generally as coating
The properties of metallic matrix components, but if being exposed in working environment for a long time, silver coating is easy by sulfide and halogen
The corrosion of the substances such as compound, makes surface change colour, and influences its properties of product.
The protection of silver at present can effectively improve the anti-corrosion of silver mainly using chemical passivation and electrochemical passivation as major way
Performance.But the modes such as plating can generate a large amount of waste water, pollute environment.Thus, it is contemplated that the factors such as environmental protection, high-efficiency environment friendly
Silver protecting agent is current research hotspot.Since electronic connector is in the process of work, due between workpiece, tool, electric wire
Friction is easily destroyed or peels off the protective layer of silver protecting agent formation.The adhesion property of silver protecting agent in the prior art is not high,
So that this defect is especially prominent.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of water base silver protecting agent, and adhesion property is good, and stability is higher, is not easy
It is destroyed or peels off, guard time greatly prolongs.
The second object of the present invention is to provide a kind of protectant preparation method of water based silver, easy to operate, at low cost,
Industrialization production easy to accomplish, the silver protecting agent stability of acquisition is high, adhesive force is strong.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of water base silver protecting agent, every liter of water base silver protecting agent include:
Stearyl mercaptan 40-60g, trimethyl sulfydryl phosphate 4-10g, emulsifier 20-60g, coupling agent 2-5g, two
Silica 5-10g, stabilizer 10-15g, surplus are water.
Preferably, the emulsifier be OP-10, ethoxylated dodecyl alcohol, one in isomerous tridecanol polyoxyethylene ether
Kind is a variety of.
Preferably, the coupling agent is one of KH-550, KH-570, KH-560 or a variety of.
Preferably, the stabilizer is one of isopropanol, glycerol, Succimer or a variety of.
Preferably, the silica is nano silica, partial size 10-50nm.
Optionally, every liter of water base silver protecting agent further include:
Polymethoxy dimethyl ether 2-5g, nano-titanium dioxide 1-2g, cobalt-lithium oxide 0.1-0.5g and aqueous polythiophene 0.5-
1.5g。
The degree of polymerization N of polymethoxy dimethyl ether used in this application is 3-8.
A kind of protectant preparation method of water based silver, comprising the following steps:
Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, under the conditions of the first temperature, with First Speed
It is mixed to get component A；
Coupling agent and silica are added to the water, are mixed to get B component under the conditions of second temperature, with second speed；
Emulsifier and stabilizer are added to the water, are mixed to get component C under the conditions of third temperature, with third speed；
Component A, B component, component C are mixed, stir to get the water base silver protecting agent.
Preferably, the preparation method is further comprising the steps of:
Polymethoxy dimethyl ether, nano-titanium dioxide, cobalt-lithium oxide and aqueous polythiophene are mixed to get component D, then
The component D is added in the mixture of the component A, the B component, the component C, stirs to get the water based silver and protect
Protect agent.
Preferably, method component A, B component, component C mixed are as follows:
The component B is at the uniform velocity added drop-wise in the component A, then at 40-50 DEG C by the first stage under keeping warm mode
0.5-1h is kept the temperature, 20 DEG C is cooled to according still further to 5-10 DEG C/min and obtains intermediate blend；
Component C is at the uniform velocity added drop-wise in the intermediate blend under keeping warm mode, then heats to 60 by second stage
DEG C heat preservation 10-20min, be cooled to 20 DEG C according still further to 1-2 DEG C/min.
Optionally, first temperature, the second temperature and the third temperature are 55-60 DEG C；First speed
Degree, the second speed and the third speed are 800-1000r/min.
Compared with prior art, the invention has the benefit that
(1) adhesive force is strong, and wearability is good；
(2) guard time of component is greatly prolonged；
(3) the protectant stability of the water based silver being prepared is good.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described reality
Applying example is only a part of the embodiments of the present invention, instead of all the embodiments.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention, based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.The person that is not specified actual conditions in embodiment, according to conventional conditions or manufacturer's recommended conditions into
Row.Reagents or instruments used without specified manufacturer is the conventional products that can be obtained by commercially available purchase.
It is to be appreciated that if relating to the description of " first ", " second " etc. in the embodiment of the present invention, " first ", " the
Two " etc. description is used for description purposes only, and is not understood to indicate or imply its relative importance or is implicitly indicated meaning
The quantity of the technical characteristic shown." first " is defined as a result, the feature of " second " can explicitly or implicitly include at least
One this feature.It in addition, the technical solution between each embodiment can be combined with each other, but must be common with this field
Based on technical staff can be realized, it will be understood that when the combination of technical solution appearance is conflicting or cannot achieve this
The combination of technical solution is not present, also not the present invention claims protection scope within.
Embodiment 1
Take Stearyl mercaptan 40g, trimethyl sulfydryl phosphate 10g, OP-10 emulsifier 20g, KH-550 coupling agent 5g,
Partial size is the nano silica 10g of 10nm, isopropanol 10g, spare.
Above-mentioned Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, under the conditions of 55 DEG C, with 1000r/min
Speed be mixed and obtain component A in 1 hour；
KH-550 and nano silica are added to the water, are mixed under the conditions of 60 DEG C, with the speed of 800r/min
Obtain B component within 2 hours；
OP-10 and isopropanol are added to the water, are mixed 1 hour under the conditions of 55 DEG C, with the speed of 1000r/min
Obtain component C；
Component A, B component, component C are mixed, stirring obtains the water base silver protecting agent of 1L in 1 hour.
Embodiment 2
Take Stearyl mercaptan 60g, trimethyl sulfydryl phosphate 4g, ethoxylated dodecyl alcohol 60g, KH-570 coupling
Agent 2g, the nano silica 5g that partial size is 50nm, glycerol 15g, polymethoxy dimethyl ether 2g, nano-titanium dioxide 2g, oxidation
Cobalt lithium 0.1g and aqueous polythiophene 1.5g, it is spare.
Above-mentioned Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, under the conditions of 60 DEG C, with 800r/min
Speed be mixed and obtain component A in 1 hour；
KH-570 and nano silica are added to the water, are mixed under the conditions of 58 DEG C, with the speed of 900r/min
Obtain B component within 2 hours；
Ethoxylated dodecyl alcohol and glycerol are added to the water, stirred under the conditions of 60 DEG C, with the speed mixing of 800r/min
It mixes 1 hour and obtains component C；
Component A, B component, component C are mixed, by polymethoxy dimethyl ether, nano-titanium dioxide, cobalt-lithium oxide and aqueous
Polythiophene is mixed to get component D, then component D is added in the mixture of component A, B component, component C, and stirring obtains for 1 hour
The water base silver protecting agent of 1L.
Embodiment 3
Take Stearyl mercaptan 50g, trimethyl sulfydryl phosphate 6g, isomerous tridecanol polyoxyethylene ether 60g, KH-560
Coupling agent 3g, nano silica 8g, Succimer 12g, the polymethoxy dimethyl ether 5g, nano-silica that partial size is 30nm
Change titanium 1g, cobalt-lithium oxide 0.5g and aqueous polythiophene 0.5g, it is spare.
Above-mentioned Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, under the conditions of 58 DEG C, with 900r/min
Speed be mixed to get component A；
KH-560 and nano silica are added to the water, mixed under the conditions of 55 DEG C, with the speed of 1000r/min
To B component；
Isomerous tridecanol polyoxyethylene ether and Succimer are added to the water, under the conditions of 58 DEG C, with 900r/min's
Speed is mixed to get component C；
Component B is at the uniform velocity added drop-wise in component A by the first stage under keeping warm mode under the mixing speed of 400r/min,
Then in 40 DEG C of heat preservation 1h, 20 DEG C is cooled to according still further to 5 DEG C/min and obtains intermediate blend；Second stage, under keeping warm mode
Component C is at the uniform velocity added drop-wise in intermediate blend under the mixing speed of 400r/min, then heats to 60 DEG C of heat preservation 20min,
20 DEG C are cooled to according still further to 1 DEG C/min；
Polymethoxy dimethyl ether, nano-titanium dioxide, cobalt-lithium oxide and aqueous polythiophene are mixed to get component D, then
Component D is added in the mixture of component A, B component, component C, stirs to get the water base silver protecting agent of 1L.
Embodiment 4
Take Stearyl mercaptan 45g, trimethyl sulfydryl phosphate 8g, isomerous tridecanol polyoxyethylene ether 40g, KH-550
Coupling agent 4g, nano silica 6g, glycerol 14g, the polymethoxy dimethyl ether 3g, nano-titanium dioxide that partial size is 40nm
1.5g, cobalt-lithium oxide 0.4g and aqueous polythiophene 1g, it is spare.
Above-mentioned Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, under the conditions of 55 DEG C, with 900r/min
Speed be mixed to get component A；
KH-550 and nano silica are added to the water, are mixed to get under the conditions of 55 DEG C, with the speed of 900r/min
B component；
Isomerous tridecanol polyoxyethylene ether and Succimer are added to the water, under the conditions of 55 DEG C, with 900r/min's
Speed is mixed to get component C；
Component B is at the uniform velocity added drop-wise in component A by the first stage under keeping warm mode under the mixing speed of 400r/min,
Then in 50 DEG C of heat preservation 0.5h, 20 DEG C is cooled to according still further to 10 DEG C/min and obtains intermediate blend；Second stage, in heat preservation shape
Component C is at the uniform velocity added drop-wise in intermediate blend under the mixing speed of 400r/min under state, then heats to 60 DEG C of heat preservations
10min is cooled to 20 DEG C according still further to 2 DEG C/min；
Polymethoxy dimethyl ether, nano-titanium dioxide, cobalt-lithium oxide and aqueous polythiophene are mixed to get component D, then
Component D is added in the mixture of component A, B component, component C, stirs to get the water base silver protecting agent of 1L.
Embodiment 5
Take Stearyl mercaptan 55g, trimethyl sulfydryl phosphate 5g, OP-10 emulsifier 30g, KH-570 coupling agent
3.5g, partial size be the nano silica 7g of 50nm, isopropanol 11g, polymethoxy dimethyl ether 4g, nano-titanium dioxide 1.8g,
Cobalt-lithium oxide 0.2g and aqueous polythiophene 1.2g, it is spare.
Above-mentioned Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, under the conditions of 60 DEG C, with 900r/min
Speed be mixed to get component A；
KH-570 and nano silica are added to the water, are mixed to get under the conditions of 60 DEG C, with the speed of 900r/min
B component；
OP-10 and isopropanol are added to the water, are mixed to get component C under the conditions of 55 DEG C, with the speed of 900r/min；
Component B is at the uniform velocity added drop-wise in component A by the first stage under keeping warm mode under the mixing speed of 400r/min,
Then in 45 DEG C of heat preservation 0.8h, 20 DEG C is cooled to according still further to 8 DEG C/min and obtains intermediate blend；Second stage, in keeping warm mode
It is lower to be at the uniform velocity added drop-wise to component C in intermediate blend under the mixing speed of 400r/min, then heat to 60 DEG C of heat preservations
15min is cooled to 20 DEG C according still further to 1.5 DEG C/min；
Polymethoxy dimethyl ether, nano-titanium dioxide, cobalt-lithium oxide and aqueous polythiophene are mixed to get component D, then
Component D is added in the mixture of component A, B component, component C, stirs to get the water base silver protecting agent of 1L.
Comparative example 1
Compared with Example 1, difference is, does not add coupling agent.
Comparative example 2
Compared with Example 2, difference is, does not add nano silica.
Comparative example 3
Compared with Example 1, difference is, does not add coupling agent and nano silica, but reduction-oxidation graphite is added
Alkene 100mg.
In order to test the protectant stability of water based silver provided by the present application and adhesion property, Example and comparative example
Resulting protective agent protects plating silver strip, carries out 30 DEG C, 5% potassium sulfide resistance test, 400 DEG C after placing a period of time
High temperature tolerance discoloration test, (potassium sulfide tolerance time is still able to maintain 15 minutes the test of validity limit time after placing N days
Above).
It is specific that test result is as follows shown in table 1:
1 test result of table
| Project | Potassium sulfide resistance results | 400 DEG C of high temperature tolerance results | Validity limit time/day |
| Embodiment 1 | Start to change colour after 30 minutes | Start to change colour after forty minutes | 260 days |
| Embodiment 2 | Start to change colour after 35 minutes | Start to change colour after 45 minutes | 275 days |
| Embodiment 3 | Start to change colour after 46 minutes | Start to change colour after 52 minutes | 352 days |
| Embodiment 4 | Start to change colour after 50 minutes | Start to change colour after 55 minutes | 350 days |
| Embodiment 5 | Start to change colour after 48 minutes | Start to change colour after 50 minutes | 348 days |
| Comparative example 1 | Start to change colour after 25 minutes | Start to change colour after twenty minutes | 180 days |
| Comparative example 2 | Start to change colour after 18 minutes | Start to change colour after 25 minutes | 200 days |
| Comparative example 3 | Start to change colour after 12 minutes | Start to change colour after twenty minutes | 175 days |
The comparison of the test data of embodiment 1 and embodiment 2 shows polymethoxy dimethyl ether, nano-titanium dioxide, oxidation
The addition of cobalt lithium and aqueous polythiophene all improves a lot to the protectant stability of water based silver, adhesive force and wearability,
This is because increasing polymethoxy dimethyl ether improves the mixed performance between each ingredient, and then its synergistic effect is improved, mixed
Miscellaneous nano-titanium dioxide and cobalt-lithium oxide improve dispersion performance, hydrophilicity and chemical stability into system, in silver and two
Transition is formed between silica；Aqueous polythiophene is added and guarantees whole bond strength, improves its adhesive force and wearability.It is real
The test data comparison for applying example 2 and embodiment 3-5 shows that preparation method provided by the present application can further improve silver-colored guarantor
The performance of agent is protected, this is because temperature, mixing speed and charging sequence and heating temperature-fall period are to ingredient each in silver protecting agent
Distribution have an impact, and then influence its overall performance；Embodiment 1 and the test result of comparative example 1 show coupling agent pair
All have a significant impact in the protectant stability of water based silver, adhesive force and wearability, this is because coupling agent hydrolysis and silver surface
The reason of forming covalent bond.Embodiment 2 and the test result of comparative example 2 show nano silica for water base silver protecting agent
Performance there is also larger impact, this is because nano silica can be formed under the action of coupling agent on the surface of silver
The transition zone of crosslinking improves the overall stability that protective agent is formed by protective layer.In order to further prove relative to
For the prior art, the advantage of the scheme of the application is ad hoc to determine comparative example 3, and test result comparison shows provided by the present application
The protectant performance of water based silver is substantially better than by Stearyl mercaptan, trimethyl sulfydryl phosphate, emulsifier, stabilizer, reduction
The protective agent of graphene oxide composition.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by present specification, or directly/it is used in it indirectly
He is included in scope of patent protection of the invention relevant technical field.
Claims (10)
1. a kind of water base silver protecting agent, which is characterized in that every liter of water base silver protecting agent includes:
Stearyl mercaptan 40-60g, trimethyl sulfydryl phosphate 4-10g, emulsifier 20-60g, coupling agent 2-5g, silica
5-10g, stabilizer 10-15g, surplus are water.
2. water base silver protecting agent according to claim 1, which is characterized in that the emulsifier is OP-10, laruyl alcohol polyoxy
One of vinethene, isomerous tridecanol polyoxyethylene ether are a variety of.
3. water base silver protecting agent according to claim 1, which is characterized in that the coupling agent be KH-550, KH-570,
One of KH-560 or a variety of.
4. water base silver protecting agent according to claim 1, which is characterized in that the stabilizer is isopropanol, glycerol, two mercaptos
One of succinic acid is a variety of.
5. water base silver protecting agent according to claim 1, which is characterized in that the silica is nano silica,
Partial size is 10-50nm.
6. water base silver protecting agent according to claim 1-5, which is characterized in that every liter of water base silver protecting agent
Further include:
Polymethoxy dimethyl ether 2-5g, nano-titanium dioxide 1-2g, cobalt-lithium oxide 0.1-0.5g and aqueous polythiophene 0.5-1.5g.
7. a kind of protectant preparation method of described in any item water based silvers of claim 1-5, which is characterized in that including following step
It is rapid:
Stearyl mercaptan, trimethyl sulfydryl phosphate are added to the water, mixed under the conditions of the first temperature, with First Speed
To component A；
Coupling agent and silica are added to the water, are mixed to get B component under the conditions of second temperature, with second speed；
Emulsifier and stabilizer are added to the water, are mixed to get component C under the conditions of third temperature, with third speed；
Component A, B component, component C are mixed, stir to get the water base silver protecting agent.
8. preparation method according to claim 7, which is characterized in that further comprising the steps of:
Polymethoxy dimethyl ether, nano-titanium dioxide, cobalt-lithium oxide and aqueous polythiophene are mixed to get component D, then by institute
It states component D to be added in the mixture of the component A, the B component, the component C, stirs to get the water base silver protecting agent.
9. preparation method according to claim 7, which is characterized in that the method for mixing component A, B component, component C are as follows:
The component B is at the uniform velocity added drop-wise in the component A by the first stage under keeping warm mode, is then kept the temperature at 40-50 DEG C
0.5-1h is cooled to 20 DEG C according still further to 5-10 DEG C/min and obtains intermediate blend；
Component C is at the uniform velocity added drop-wise in the intermediate blend by second stage under keeping warm mode, then heats to 60 DEG C of heat preservations
10-20min is cooled to 20 DEG C according still further to 1-2 DEG C/min.
10. according to the described in any item preparation methods of claim 7-9, which is characterized in that first temperature, second temperature
Degree and the third temperature are 55-60 DEG C；The First Speed, the second speed and the third speed are 800-
1000r/min。
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| CN116355452A (en) * | 2023-04-12 | 2023-06-30 | 东莞市促裕新材料有限公司 | Sulfur-resistant salt-fog-resistant metal protective agent and preparation method thereof |
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| CN110055523B (en) | 2021-05-07 |
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